Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.007 Å
- Disorder in main residue
- R factor = 0.040
- wR factor = 0.120
- Data-to-parameter ratio = 14.7
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT432_ALERT_2_A Short Inter X...Y Contact O8 .. C25 .. 1.38 Ang.
| Author Response: The 4-hydroxybenzoic acid and water molecules are disordered about a
center-of-inversion. The treatement of the disoder is described in the
refinement.
|
PLAT432_ALERT_2_A Short Inter X...Y Contact O8 .. C26 .. 2.36 Ang.
| Author Response: The 4-hydroxybenzoic acid and water molecules are disordered about a
center-of-inversion. The treatement of the disoder is described in the
refinement.
|
PLAT432_ALERT_2_A Short Inter X...Y Contact O8 .. C24 .. 2.43 Ang.
| Author Response: The 4-hydroxybenzoic acid and water molecules are disordered about a
center-of-inversion. The treatement of the disoder is described in the
refinement.
|
PLAT432_ALERT_2_A Short Inter X...Y Contact C22 .. C24 .. 2.41 Ang.
| Author Response: The 4-hydroxybenzoic acid and water molecules are disordered about a
center-of-inversion. The treatement of the disoder is described in the
refinement.
|
PLAT432_ALERT_2_A Short Inter X...Y Contact C22 .. C25 .. 2.78 Ang.
| Author Response: The 4-hydroxybenzoic acid and water molecules are disordered about a
center-of-inversion. The treatement of the disoder is described in the
refinement.
|
PLAT432_ALERT_2_A Short Inter X...Y Contact C23 .. C24 .. 1.39 Ang.
| Author Response: The 4-hydroxybenzoic acid and water molecules are disordered about a
center-of-inversion. The treatement of the disoder is described in the
refinement.
|
PLAT432_ALERT_2_A Short Inter X...Y Contact C23 .. C25 .. 2.41 Ang.
| Author Response: The 4-hydroxybenzoic acid and water molecules are disordered about a
center-of-inversion. The treatement of the disoder is described in the
refinement.
|
PLAT432_ALERT_2_A Short Inter X...Y Contact C24 .. C25 .. 1.39 Ang.
| Author Response: The 4-hydroxybenzoic acid and water molecules are disordered about a
center-of-inversion. The treatement of the disoder is described in the
refinement.
|
PLAT432_ALERT_2_A Short Inter X...Y Contact C24 .. C26 .. 2.41 Ang.
| Author Response: The 4-hydroxybenzoic acid and water molecules are disordered about a
center-of-inversion. The treatement of the disoder is described in the
refinement.
|
PLAT432_ALERT_2_A Short Inter X...Y Contact C24 .. C27 .. 2.78 Ang.
| Author Response: The 4-hydroxybenzoic acid and water molecules are disordered about a
center-of-inversion. The treatement of the disoder is described in the
refinement.
|
PLAT432_ALERT_2_A Short Inter X...Y Contact C25 .. C26 .. 1.39 Ang.
| Author Response: The 4-hydroxybenzoic acid and water molecules are disordered about a
center-of-inversion. The treatement of the disoder is described in the
refinement.
|
PLAT432_ALERT_2_A Short Inter X...Y Contact C25 .. C27 .. 2.41 Ang.
| Author Response: The 4-hydroxybenzoic acid and water molecules are disordered about a
center-of-inversion. The treatement of the disoder is described in the
refinement.
|
Alert level C
ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90
Tmin and Tmax reported: 0.542 0.852
Tmin(prime) and Tmax expected: 0.714 0.848
RR(prime) = 0.756
Please check that your absorption correction is appropriate.
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.75
PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.67 Ratio
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O1
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C13
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C1
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C22
PLAT301_ALERT_3_C Main Residue Disorder ......................... 3.00 Perc.
PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc.
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.17 Ratio
Alert level G
PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 4
12 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
11 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
17 ALERT type 2 Indicator that the structure model may be wrong or deficient
4 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Cadmium dinitrate tetrahydrate (2 mmol), 2,2'-bipyridine (2 mmol) and
3-(4-carboxylatophenoxy)propionic acid (2 mmol) and water were sealed in a
25-ml, Teflon-lined, stainless steel bomb and heated at 413 K for 20 h. The
bomb was cooled to room temperature; the colorless crystals that separated was
picked out manually.
The water and 4-hydroxybenzoic acid molecules are disordered about a
center-of-inversion; the molecules were assigned half-occupancy each. The
phenylene ring was refined as a rigid hexagon of 1.39 Å sides. The four-atom
–C(=O)–O fragment was restrained to be nearly planar; the two C–O distances
were restrained to 1.25±0.01 Å and the C–C single-bond distance to
1.50±-0.01 Å.
Carbon-bound H atoms were placed in calculated positions [C—H 0.93–0.97 Å
and Uiso(H) 1.2Ueq(C)], and were included in the refinement
in the riding-model approximation. The carboxylic acid and water H-atoms were
similarly generated [O–H 0.82 Å and and Uiso(H)
1.2Ueq(O)].
The final difference Fourier map had a large peak near Cd1, but was otherwise
essentially featureless.
Data collection: RAPID-AUTO (Rigaku Corporation, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001), OLEX (Dolomanov et al., 2003); software used to prepare material for publication: publCIF (Westrip, 2007).
Poly[[[bis[(2,2'-bipyridine-
κ2N,
N')cadmium(II)]-
bis[µ
3-3-(4-carboxylatophenoxy)propionato-
κ5O,
O':
O':
O'',
O''']] 4-hydroxybenzoic
acid monohydrate]
top
Crystal data top
[Cd2(C10H8O5)2(C10H8N2)2]·C7H6O3·H2O | Z = 1 |
Mr = 1109.63 | F(000) = 558 |
Triclinic, P1 | Dx = 1.659 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.1615 (5) Å | Cell parameters from 8754 reflections |
b = 10.6255 (5) Å | θ = 3.0–27.5° |
c = 10.8507 (6) Å | µ = 1.03 mm−1 |
α = 73.147 (2)° | T = 295 K |
β = 82.174 (1)° | Block, colorless |
γ = 88.734 (1)° | 0.32 × 0.24 × 0.16 mm |
V = 1110.6 (1) Å3 | |
Data collection top
Rigaku RAXIS-RAPID diffractometer | 5010 independent reflections |
Radiation source: fine-focus sealed tube | 3997 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.042 |
Detector resolution: 10.000 pixels mm-1 | θmax = 27.5°, θmin = 3.0° |
ω–scans | h = −13→13 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −11→13 |
Tmin = 0.542, Tmax = 0.852 | l = −14→14 |
10857 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.040 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.120 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.048P)2 + 1.4148P] where P = (Fo2 + 2Fc2)/3 |
5010 reflections | (Δ/σ)max = 0.001 |
341 parameters | Δρmax = 1.13 e Å−3 |
4 restraints | Δρmin = −0.87 e Å−3 |
Crystal data top
[Cd2(C10H8O5)2(C10H8N2)2]·C7H6O3·H2O | γ = 88.734 (1)° |
Mr = 1109.63 | V = 1110.6 (1) Å3 |
Triclinic, P1 | Z = 1 |
a = 10.1615 (5) Å | Mo Kα radiation |
b = 10.6255 (5) Å | µ = 1.03 mm−1 |
c = 10.8507 (6) Å | T = 295 K |
α = 73.147 (2)° | 0.32 × 0.24 × 0.16 mm |
β = 82.174 (1)° | |
Data collection top
Rigaku RAXIS-RAPID diffractometer | 5010 independent reflections |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | 3997 reflections with I > 2σ(I) |
Tmin = 0.542, Tmax = 0.852 | Rint = 0.042 |
10857 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.040 | 4 restraints |
wR(F2) = 0.120 | H-atom parameters constrained |
S = 1.06 | Δρmax = 1.13 e Å−3 |
5010 reflections | Δρmin = −0.87 e Å−3 |
341 parameters | |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Cd1 | 0.42672 (3) | 0.67472 (3) | 0.96257 (3) | 0.04096 (12) | |
O1 | 0.4806 (4) | 0.6852 (4) | 0.7269 (3) | 0.0713 (11) | |
O2 | 0.4891 (3) | 0.5017 (3) | 0.8745 (3) | 0.0503 (7) | |
O3 | 0.7194 (3) | 0.5162 (4) | 0.4709 (3) | 0.0528 (8) | |
O4 | 1.2813 (3) | 0.7051 (3) | 0.1393 (3) | 0.0524 (8) | |
O5 | 1.1998 (3) | 0.6081 (3) | 0.0120 (3) | 0.0501 (8) | |
N1 | 0.6322 (3) | 0.7835 (4) | 0.9263 (3) | 0.0422 (8) | |
N2 | 0.3986 (3) | 0.8980 (4) | 0.8686 (4) | 0.0506 (9) | |
C1 | 0.5078 (4) | 0.5672 (5) | 0.7584 (4) | 0.0423 (10) | |
C2 | 0.5637 (4) | 0.5052 (6) | 0.6544 (4) | 0.0544 (12) | |
H2A | 0.4973 | 0.5069 | 0.5976 | 0.065* | |
H2B | 0.5831 | 0.4139 | 0.6948 | 0.065* | |
C3 | 0.6886 (4) | 0.5747 (5) | 0.5741 (4) | 0.0501 (11) | |
H3A | 0.6738 | 0.6681 | 0.5399 | 0.060* | |
H3B | 0.7606 | 0.5627 | 0.6264 | 0.060* | |
C4 | 0.8339 (4) | 0.5545 (4) | 0.3857 (4) | 0.0366 (8) | |
C5 | 0.9291 (4) | 0.6386 (5) | 0.4003 (4) | 0.0470 (10) | |
H5 | 0.9163 | 0.6751 | 0.4692 | 0.056* | |
C6 | 1.0433 (4) | 0.6675 (5) | 0.3111 (4) | 0.0450 (10) | |
H6 | 1.1087 | 0.7219 | 0.3218 | 0.054* | |
C7 | 1.0620 (4) | 0.6166 (4) | 0.2057 (4) | 0.0357 (8) | |
C8 | 0.9646 (4) | 0.5349 (4) | 0.1924 (4) | 0.0407 (9) | |
H8 | 0.9758 | 0.4997 | 0.1227 | 0.049* | |
C9 | 0.8502 (4) | 0.5047 (5) | 0.2819 (4) | 0.0466 (10) | |
H9 | 0.7846 | 0.4506 | 0.2712 | 0.056* | |
C10 | 1.1891 (4) | 0.6454 (4) | 0.1128 (4) | 0.0383 (9) | |
C11 | 0.7459 (4) | 0.7223 (5) | 0.9483 (5) | 0.0507 (11) | |
H11 | 0.7436 | 0.6317 | 0.9860 | 0.061* | |
C12 | 0.8668 (5) | 0.7873 (6) | 0.9178 (6) | 0.0690 (15) | |
H12 | 0.9449 | 0.7416 | 0.9333 | 0.083* | |
C13 | 0.8693 (5) | 0.9193 (6) | 0.8645 (8) | 0.096 (3) | |
H13 | 0.9498 | 0.9657 | 0.8426 | 0.115* | |
C14 | 0.7518 (5) | 0.9853 (5) | 0.8427 (7) | 0.0749 (18) | |
H14 | 0.7521 | 1.0764 | 0.8090 | 0.090* | |
C15 | 0.6343 (4) | 0.9139 (4) | 0.8718 (4) | 0.0405 (9) | |
C16 | 0.5054 (4) | 0.9786 (4) | 0.8424 (4) | 0.0391 (9) | |
C17 | 0.4953 (5) | 1.1124 (5) | 0.7919 (5) | 0.0555 (12) | |
H17 | 0.5702 | 1.1667 | 0.7754 | 0.067* | |
C18 | 0.3730 (5) | 1.1661 (5) | 0.7658 (6) | 0.0638 (14) | |
H18 | 0.3644 | 1.2565 | 0.7322 | 0.077* | |
C19 | 0.2654 (5) | 1.0838 (6) | 0.7902 (6) | 0.0750 (17) | |
H19 | 0.1825 | 1.1169 | 0.7717 | 0.090* | |
C20 | 0.2812 (5) | 0.9547 (5) | 0.8413 (6) | 0.0717 (17) | |
H20 | 0.2064 | 0.9001 | 0.8594 | 0.086* | |
O1w | 0.6482 (8) | 1.1595 (8) | 0.4750 (9) | 0.077 (2) | 0.50 |
H1w | 0.6162 | 1.2113 | 0.4151 | 0.092* | 0.50 |
H2w | 0.6057 | 1.0901 | 0.4959 | 0.092* | 0.50 |
O6 | −0.1473 (12) | 0.9220 (11) | 0.5206 (16) | 0.089 (4) | 0.50 |
O7 | −0.1003 (11) | 1.1321 (8) | 0.4495 (14) | 0.078 (5) | 0.50 |
H7O | −0.1790 | 1.1487 | 0.4448 | 0.117* | 0.50 |
O8 | 0.4798 (7) | 0.9246 (7) | 0.5287 (8) | 0.0657 (19) | 0.50 |
H8O | 0.4907 | 0.8528 | 0.5804 | 0.099* | 0.50 |
C21 | −0.0645 (10) | 1.0142 (12) | 0.4888 (14) | 0.071 (8) | 0.50 |
C22 | 0.0799 (7) | 0.9884 (13) | 0.4960 (19) | 0.059 (6) | 0.50 |
C23 | 0.1194 (8) | 0.8635 (11) | 0.5611 (16) | 0.127 (14) | 0.50 |
H23 | 0.0564 | 0.7964 | 0.5983 | 0.153* | 0.50 |
C24 | 0.2532 (9) | 0.8391 (6) | 0.5707 (10) | 0.074 (3) | 0.50 |
H24 | 0.2796 | 0.7555 | 0.6143 | 0.089* | 0.50 |
C25 | 0.3473 (6) | 0.9395 (7) | 0.5152 (8) | 0.054 (2) | 0.50 |
C26 | 0.3077 (8) | 1.0643 (6) | 0.4500 (8) | 0.055 (2) | 0.50 |
H26 | 0.3707 | 1.1315 | 0.4128 | 0.066* | 0.50 |
C27 | 0.1740 (9) | 1.0888 (9) | 0.4404 (14) | 0.066 (5) | 0.50 |
H27 | 0.1476 | 1.1724 | 0.3968 | 0.079* | 0.50 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd1 | 0.03119 (16) | 0.04466 (19) | 0.04179 (19) | −0.00141 (12) | 0.00713 (11) | −0.00967 (14) |
O1 | 0.081 (2) | 0.080 (3) | 0.040 (2) | 0.030 (2) | 0.0032 (17) | −0.0039 (18) |
O2 | 0.0553 (17) | 0.0601 (19) | 0.0309 (16) | 0.0082 (15) | 0.0077 (13) | −0.0127 (14) |
O3 | 0.0361 (15) | 0.083 (2) | 0.0409 (17) | −0.0108 (15) | 0.0124 (12) | −0.0284 (17) |
O4 | 0.0339 (15) | 0.066 (2) | 0.058 (2) | −0.0112 (15) | 0.0079 (13) | −0.0255 (17) |
O5 | 0.0414 (16) | 0.064 (2) | 0.0483 (18) | −0.0108 (15) | 0.0130 (13) | −0.0295 (16) |
N1 | 0.0361 (17) | 0.046 (2) | 0.044 (2) | 0.0026 (15) | −0.0018 (14) | −0.0144 (16) |
N2 | 0.0370 (18) | 0.051 (2) | 0.057 (2) | −0.0029 (17) | 0.0016 (16) | −0.0078 (19) |
C1 | 0.0290 (18) | 0.063 (3) | 0.035 (2) | 0.0069 (19) | −0.0027 (15) | −0.015 (2) |
C2 | 0.039 (2) | 0.091 (4) | 0.033 (2) | −0.005 (2) | 0.0071 (17) | −0.022 (2) |
C3 | 0.037 (2) | 0.077 (3) | 0.035 (2) | 0.003 (2) | 0.0047 (17) | −0.018 (2) |
C4 | 0.0277 (17) | 0.045 (2) | 0.034 (2) | 0.0036 (16) | 0.0028 (14) | −0.0099 (17) |
C5 | 0.038 (2) | 0.065 (3) | 0.042 (2) | 0.004 (2) | 0.0039 (17) | −0.025 (2) |
C6 | 0.035 (2) | 0.058 (3) | 0.045 (2) | −0.0091 (19) | 0.0054 (17) | −0.025 (2) |
C7 | 0.0322 (18) | 0.036 (2) | 0.036 (2) | 0.0016 (16) | 0.0032 (15) | −0.0087 (17) |
C8 | 0.041 (2) | 0.048 (2) | 0.034 (2) | −0.0034 (18) | 0.0062 (16) | −0.0185 (18) |
C9 | 0.037 (2) | 0.059 (3) | 0.046 (3) | −0.011 (2) | 0.0058 (17) | −0.022 (2) |
C10 | 0.0299 (18) | 0.038 (2) | 0.043 (2) | 0.0038 (16) | 0.0025 (16) | −0.0093 (18) |
C11 | 0.043 (2) | 0.046 (2) | 0.060 (3) | 0.006 (2) | −0.010 (2) | −0.010 (2) |
C12 | 0.039 (2) | 0.063 (3) | 0.102 (5) | 0.004 (2) | −0.010 (3) | −0.020 (3) |
C13 | 0.039 (3) | 0.063 (4) | 0.176 (8) | −0.007 (3) | −0.012 (4) | −0.019 (4) |
C14 | 0.047 (3) | 0.040 (3) | 0.126 (6) | −0.002 (2) | −0.010 (3) | −0.009 (3) |
C15 | 0.040 (2) | 0.038 (2) | 0.045 (2) | 0.0003 (17) | −0.0021 (17) | −0.0174 (19) |
C16 | 0.044 (2) | 0.039 (2) | 0.034 (2) | 0.0084 (18) | −0.0026 (16) | −0.0125 (17) |
C17 | 0.057 (3) | 0.041 (2) | 0.068 (3) | 0.002 (2) | −0.014 (2) | −0.013 (2) |
C18 | 0.064 (3) | 0.055 (3) | 0.067 (4) | 0.010 (3) | −0.018 (3) | −0.005 (3) |
C19 | 0.051 (3) | 0.074 (4) | 0.084 (4) | 0.017 (3) | −0.022 (3) | 0.007 (3) |
C20 | 0.042 (2) | 0.055 (3) | 0.104 (5) | 0.003 (2) | −0.017 (3) | 0.002 (3) |
O1w | 0.071 (5) | 0.061 (5) | 0.082 (6) | 0.008 (5) | −0.024 (5) | 0.011 (4) |
O6 | 0.068 (6) | 0.077 (8) | 0.132 (12) | 0.000 (6) | −0.044 (8) | −0.032 (7) |
O7 | 0.065 (6) | 0.035 (5) | 0.134 (13) | 0.010 (5) | −0.022 (7) | −0.021 (7) |
O8 | 0.060 (4) | 0.060 (4) | 0.066 (5) | 0.003 (4) | −0.008 (3) | 0.000 (4) |
C21 | 0.068 (10) | 0.069 (19) | 0.082 (17) | 0.005 (11) | −0.027 (10) | −0.025 (13) |
C22 | 0.059 (10) | 0.065 (17) | 0.053 (10) | −0.009 (10) | −0.011 (8) | −0.013 (10) |
C23 | 0.12 (2) | 0.14 (2) | 0.092 (18) | −0.026 (17) | −0.050 (17) | 0.025 (16) |
C24 | 0.069 (7) | 0.048 (6) | 0.098 (10) | 0.004 (6) | −0.035 (7) | 0.000 (6) |
C25 | 0.062 (6) | 0.050 (6) | 0.044 (5) | 0.002 (5) | −0.007 (4) | −0.004 (5) |
C26 | 0.060 (6) | 0.044 (5) | 0.056 (6) | 0.003 (4) | −0.004 (5) | −0.009 (4) |
C27 | 0.079 (11) | 0.045 (8) | 0.066 (9) | 0.001 (7) | −0.007 (7) | −0.004 (6) |
Geometric parameters (Å, º) top
Cd1—O1 | 2.511 (4) | C9—H9 | 0.9300 |
Cd1—O2 | 2.345 (3) | C11—C12 | 1.375 (7) |
Cd1—O2i | 2.406 (3) | C11—H11 | 0.9300 |
Cd1—O4ii | 2.351 (3) | C12—C13 | 1.353 (8) |
Cd1—O5ii | 2.370 (3) | C12—H12 | 0.9300 |
Cd1—N1 | 2.339 (3) | C13—C14 | 1.385 (7) |
Cd1—N2 | 2.323 (4) | C13—H13 | 0.9300 |
O1—C1 | 1.236 (6) | C14—C15 | 1.378 (6) |
O2—C1 | 1.241 (5) | C14—H14 | 0.9300 |
O2—Cd1i | 2.406 (3) | C15—C16 | 1.496 (6) |
O3—C4 | 1.373 (4) | C16—C17 | 1.375 (6) |
O3—C3 | 1.428 (5) | C17—C18 | 1.387 (7) |
O4—C10 | 1.253 (5) | C17—H17 | 0.9300 |
O4—Cd1iii | 2.351 (3) | C18—C19 | 1.363 (8) |
O5—C10 | 1.257 (5) | C18—H18 | 0.9300 |
O5—Cd1iii | 2.370 (3) | C19—C20 | 1.338 (8) |
N1—C11 | 1.329 (5) | C19—H19 | 0.9300 |
N1—C15 | 1.339 (5) | C20—H20 | 0.9300 |
N2—C16 | 1.345 (5) | O1w—H1w | 0.8200 |
N2—C20 | 1.354 (6) | O1w—H2w | 0.8200 |
C1—C2 | 1.507 (6) | O6—C21 | 1.244 (9) |
C2—C3 | 1.511 (6) | O7—C21 | 1.263 (9) |
C2—H2A | 0.9700 | O7—H7O | 0.8200 |
C2—H2B | 0.9700 | O8—C25 | 1.375 (9) |
C3—H3A | 0.9700 | O8—H8O | 0.8200 |
C3—H3B | 0.9700 | C21—C22 | 1.495 (8) |
C4—C9 | 1.366 (6) | C22—C23 | 1.3900 |
C4—C5 | 1.386 (6) | C22—C27 | 1.3900 |
C5—C6 | 1.385 (5) | C23—C24 | 1.3900 |
C5—H5 | 0.9300 | C23—H23 | 0.9300 |
C6—C7 | 1.390 (6) | C24—C25 | 1.3900 |
C6—H6 | 0.9300 | C24—H24 | 0.9300 |
C7—C8 | 1.379 (6) | C25—C26 | 1.3900 |
C7—C10 | 1.505 (5) | C26—C27 | 1.3900 |
C8—C9 | 1.388 (5) | C26—H26 | 0.9300 |
C8—H8 | 0.9300 | C27—H27 | 0.9300 |
| | | |
N2—Cd1—N1 | 71.09 (12) | C7—C8—H8 | 119.6 |
N2—Cd1—O2 | 132.62 (13) | C9—C8—H8 | 119.6 |
N1—Cd1—O2 | 99.56 (12) | C4—C9—C8 | 120.0 (4) |
N2—Cd1—O4ii | 84.69 (13) | C4—C9—H9 | 120.0 |
N1—Cd1—O4ii | 114.25 (11) | C8—C9—H9 | 120.0 |
O2—Cd1—O4ii | 137.28 (11) | O4—C10—O5 | 122.2 (4) |
N2—Cd1—O5ii | 98.40 (12) | O4—C10—C7 | 118.6 (4) |
N1—Cd1—O5ii | 166.81 (11) | O5—C10—C7 | 119.2 (4) |
O2—Cd1—O5ii | 93.44 (11) | N1—C11—C12 | 122.8 (5) |
O4ii—Cd1—O5ii | 55.46 (10) | N1—C11—H11 | 118.6 |
N2—Cd1—O2i | 150.29 (13) | C12—C11—H11 | 118.6 |
N1—Cd1—O2i | 88.75 (12) | C13—C12—C11 | 118.3 (5) |
O2—Cd1—O2i | 70.79 (12) | C13—C12—H12 | 120.9 |
O4ii—Cd1—O2i | 84.10 (11) | C11—C12—H12 | 120.9 |
O5ii—Cd1—O2i | 97.67 (11) | C12—C13—C14 | 119.9 (5) |
N2—Cd1—O1 | 80.37 (14) | C12—C13—H13 | 120.1 |
N1—Cd1—O1 | 83.43 (13) | C14—C13—H13 | 120.1 |
O2—Cd1—O1 | 52.26 (12) | C15—C14—C13 | 118.9 (5) |
O4ii—Cd1—O1 | 151.63 (12) | C15—C14—H14 | 120.5 |
O5ii—Cd1—O1 | 103.05 (12) | C13—C14—H14 | 120.5 |
O2i—Cd1—O1 | 119.78 (11) | N1—C15—C14 | 120.9 (4) |
C1—O1—Cd1 | 89.9 (3) | N1—C15—C16 | 117.7 (4) |
C1—O2—Cd1 | 97.7 (3) | C14—C15—C16 | 121.4 (4) |
C1—O2—Cd1i | 144.3 (3) | N2—C16—C17 | 121.5 (4) |
Cd1—O2—Cd1i | 109.21 (12) | N2—C16—C15 | 116.1 (4) |
C4—O3—C3 | 119.1 (3) | C17—C16—C15 | 122.5 (4) |
C10—O4—Cd1iii | 91.5 (2) | C16—C17—C18 | 119.6 (5) |
C10—O5—Cd1iii | 90.5 (2) | C16—C17—H17 | 120.2 |
C11—N1—C15 | 119.2 (4) | C18—C17—H17 | 120.2 |
C11—N1—Cd1 | 123.7 (3) | C19—C18—C17 | 118.8 (5) |
C15—N1—Cd1 | 116.9 (3) | C19—C18—H18 | 120.6 |
C16—N2—C20 | 116.9 (4) | C17—C18—H18 | 120.6 |
C16—N2—Cd1 | 118.1 (3) | C20—C19—C18 | 118.8 (5) |
C20—N2—Cd1 | 124.9 (3) | C20—C19—H19 | 120.6 |
O1—C1—O2 | 119.9 (4) | C18—C19—H19 | 120.6 |
O1—C1—C2 | 119.1 (4) | C19—C20—N2 | 124.5 (5) |
O2—C1—C2 | 121.0 (4) | C19—C20—H20 | 117.8 |
C1—C2—C3 | 112.5 (4) | N2—C20—H20 | 117.8 |
C1—C2—H2A | 109.1 | H1w—O1w—H2w | 108.2 |
C3—C2—H2A | 109.1 | C21—O7—H7O | 120.0 |
C1—C2—H2B | 109.1 | O6—C21—O7 | 120.8 (10) |
C3—C2—H2B | 109.1 | O6—C21—C22 | 120.9 (9) |
H2A—C2—H2B | 107.8 | O7—C21—C22 | 118.2 (10) |
O3—C3—C2 | 105.8 (4) | C23—C22—C27 | 120.0 |
O3—C3—H3A | 110.6 | C23—C22—C21 | 119.5 (6) |
C2—C3—H3A | 110.6 | C27—C22—C21 | 120.5 (6) |
O3—C3—H3B | 110.6 | C22—C23—C24 | 120.0 |
C2—C3—H3B | 110.6 | C22—C23—H23 | 120.0 |
H3A—C3—H3B | 108.7 | C24—C23—H23 | 120.0 |
C9—C4—O3 | 115.8 (4) | C25—C24—C23 | 120.0 |
C9—C4—C5 | 120.5 (4) | C25—C24—H24 | 120.0 |
O3—C4—C5 | 123.7 (4) | C23—C24—H24 | 120.0 |
C6—C5—C4 | 119.1 (4) | O8—C25—C26 | 116.9 (6) |
C6—C5—H5 | 120.4 | O8—C25—C24 | 123.0 (6) |
C4—C5—H5 | 120.4 | C26—C25—C24 | 120.0 |
C5—C6—C7 | 121.0 (4) | C25—C26—C27 | 120.0 |
C5—C6—H6 | 119.5 | C25—C26—H26 | 120.0 |
C7—C6—H6 | 119.5 | C27—C26—H26 | 120.0 |
C8—C7—C6 | 118.6 (3) | C26—C27—C22 | 120.0 |
C8—C7—C10 | 121.3 (4) | C26—C27—H27 | 120.0 |
C6—C7—C10 | 120.0 (4) | C22—C27—H27 | 120.0 |
C7—C8—C9 | 120.8 (4) | | |
| | | |
N2—Cd1—O1—C1 | 176.3 (3) | C4—C5—C6—C7 | 1.8 (7) |
N1—Cd1—O1—C1 | 104.5 (3) | C5—C6—C7—C8 | −0.7 (7) |
O2—Cd1—O1—C1 | −3.0 (2) | C5—C6—C7—C10 | −177.8 (4) |
O4ii—Cd1—O1—C1 | −124.5 (3) | C6—C7—C8—C9 | 0.3 (7) |
O5ii—Cd1—O1—C1 | −87.2 (3) | C10—C7—C8—C9 | 177.3 (4) |
O2i—Cd1—O1—C1 | 19.7 (3) | O3—C4—C9—C8 | −178.2 (4) |
N2—Cd1—O2—C1 | 2.2 (3) | C5—C4—C9—C8 | 2.1 (7) |
N1—Cd1—O2—C1 | −70.9 (3) | C7—C8—C9—C4 | −1.0 (7) |
O4ii—Cd1—O2—C1 | 146.4 (2) | Cd1iii—O4—C10—O5 | −6.1 (4) |
O5ii—Cd1—O2—C1 | 106.9 (3) | Cd1iii—O4—C10—C7 | 173.3 (3) |
O2i—Cd1—O2—C1 | −156.2 (3) | Cd1iii—O5—C10—O4 | 6.0 (4) |
O1—Cd1—O2—C1 | 3.0 (2) | Cd1iii—O5—C10—C7 | −173.3 (3) |
N2—Cd1—O2—Cd1i | 158.33 (13) | C8—C7—C10—O4 | −170.3 (4) |
N1—Cd1—O2—Cd1i | 85.29 (14) | C6—C7—C10—O4 | 6.7 (6) |
O4ii—Cd1—O2—Cd1i | −57.5 (2) | C8—C7—C10—O5 | 9.1 (6) |
O5ii—Cd1—O2—Cd1i | −96.93 (14) | C6—C7—C10—O5 | −173.9 (4) |
O2i—Cd1—O2—Cd1i | 0.0 | C15—N1—C11—C12 | 0.2 (7) |
O1—Cd1—O2—Cd1i | 159.2 (2) | Cd1—N1—C11—C12 | 175.3 (4) |
N2—Cd1—N1—C11 | −175.4 (4) | N1—C11—C12—C13 | 0.8 (9) |
O2—Cd1—N1—C11 | −43.5 (4) | C11—C12—C13—C14 | 0.2 (11) |
O4ii—Cd1—N1—C11 | 109.8 (4) | C12—C13—C14—C15 | −2.2 (12) |
O5ii—Cd1—N1—C11 | 146.3 (5) | C11—N1—C15—C14 | −2.3 (7) |
O2i—Cd1—N1—C11 | 26.8 (4) | Cd1—N1—C15—C14 | −177.7 (4) |
O1—Cd1—N1—C11 | −93.4 (4) | C11—N1—C15—C16 | 177.0 (4) |
N2—Cd1—N1—C15 | −0.2 (3) | Cd1—N1—C15—C16 | 1.6 (5) |
O2—Cd1—N1—C15 | 131.7 (3) | C13—C14—C15—N1 | 3.3 (9) |
O4ii—Cd1—N1—C15 | −75.1 (3) | C13—C14—C15—C16 | −176.0 (6) |
O5ii—Cd1—N1—C15 | −38.5 (7) | C20—N2—C16—C17 | 0.8 (7) |
O2i—Cd1—N1—C15 | −158.0 (3) | Cd1—N2—C16—C17 | −177.2 (3) |
O1—Cd1—N1—C15 | 81.8 (3) | C20—N2—C16—C15 | −179.3 (5) |
N1—Cd1—N2—C16 | −1.4 (3) | Cd1—N2—C16—C15 | 2.6 (5) |
O2—Cd1—N2—C16 | −87.0 (3) | N1—C15—C16—N2 | −2.9 (6) |
O4ii—Cd1—N2—C16 | 116.5 (3) | C14—C15—C16—N2 | 176.5 (5) |
O5ii—Cd1—N2—C16 | 170.4 (3) | N1—C15—C16—C17 | 177.0 (4) |
O2i—Cd1—N2—C16 | 48.3 (4) | C14—C15—C16—C17 | −3.7 (7) |
O1—Cd1—N2—C16 | −87.7 (3) | N2—C16—C17—C18 | −0.8 (7) |
N1—Cd1—N2—C20 | −179.2 (5) | C15—C16—C17—C18 | 179.4 (5) |
O2—Cd1—N2—C20 | 95.2 (5) | C16—C17—C18—C19 | −0.4 (8) |
O4ii—Cd1—N2—C20 | −61.3 (5) | C17—C18—C19—C20 | 1.5 (10) |
O5ii—Cd1—N2—C20 | −7.4 (5) | C18—C19—C20—N2 | −1.5 (11) |
O2i—Cd1—N2—C20 | −129.5 (5) | C16—N2—C20—C19 | 0.3 (9) |
O1—Cd1—N2—C20 | 94.5 (5) | Cd1—N2—C20—C19 | 178.2 (5) |
Cd1—O1—C1—O2 | 5.2 (4) | O6—C21—C22—C23 | −12.1 (9) |
Cd1—O1—C1—C2 | −174.7 (3) | O7—C21—C22—C23 | 167.9 (9) |
Cd1—O2—C1—O1 | −5.6 (4) | O6—C21—C22—C27 | 169.2 (9) |
Cd1i—O2—C1—O1 | −144.9 (4) | O7—C21—C22—C27 | −10.8 (9) |
Cd1—O2—C1—C2 | 174.3 (3) | C27—C22—C23—C24 | 0.0 |
Cd1i—O2—C1—C2 | 35.1 (7) | C21—C22—C23—C24 | −178.7 (10) |
O1—C1—C2—C3 | 56.4 (6) | C22—C23—C24—C25 | 0.0 |
O2—C1—C2—C3 | −123.5 (5) | C23—C24—C25—O8 | 175.3 (10) |
C4—O3—C3—C2 | −176.0 (4) | C23—C24—C25—C26 | 0.0 |
C1—C2—C3—O3 | −172.8 (4) | O8—C25—C26—C27 | −175.6 (10) |
C3—O3—C4—C9 | −173.5 (4) | C24—C25—C26—C27 | 0.0 |
C3—O3—C4—C5 | 6.2 (6) | C25—C26—C27—C22 | 0.0 |
C9—C4—C5—C6 | −2.5 (7) | C23—C22—C27—C26 | 0.0 |
O3—C4—C5—C6 | 177.8 (4) | C21—C22—C27—C26 | 178.7 (10) |
Symmetry codes: (i) −x+1, −y+1, −z+2; (ii) x−1, y, z+1; (iii) x+1, y, z−1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O7—H7o···O1wiv | 0.82 | 1.75 | 2.55 (1) | 166 |
O8—H8o···O1 | 0.82 | 2.01 | 2.815 (8) | 168 |
O1w—H1w···O1v | 0.82 | 1.98 | 2.797 (8) | 171 |
O1w—H2w···O8 | 0.82 | 2.11 | 2.93 (1) | 172 |
Symmetry codes: (iv) x−1, y, z; (v) −x+1, −y+2, −z+1. |
Experimental details
Crystal data |
Chemical formula | [Cd2(C10H8O5)2(C10H8N2)2]·C7H6O3·H2O |
Mr | 1109.63 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 295 |
a, b, c (Å) | 10.1615 (5), 10.6255 (5), 10.8507 (6) |
α, β, γ (°) | 73.147 (2), 82.174 (1), 88.734 (1) |
V (Å3) | 1110.6 (1) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 1.03 |
Crystal size (mm) | 0.32 × 0.24 × 0.16 |
|
Data collection |
Diffractometer | Rigaku RAXIS-RAPID diffractometer |
Absorption correction | Multi-scan (ABSCOR; Higashi, 1995) |
Tmin, Tmax | 0.542, 0.852 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 10857, 5010, 3997 |
Rint | 0.042 |
(sin θ/λ)max (Å−1) | 0.649 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.040, 0.120, 1.06 |
No. of reflections | 5010 |
No. of parameters | 341 |
No. of restraints | 4 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.13, −0.87 |
Selected bond lengths (Å) topCd1—O1 | 2.511 (4) | Cd1—O5ii | 2.370 (3) |
Cd1—O2 | 2.345 (3) | Cd1—N1 | 2.339 (3) |
Cd1—O2i | 2.406 (3) | Cd1—N2 | 2.323 (4) |
Cd1—O4ii | 2.351 (3) | | |
Symmetry codes: (i) −x+1, −y+1, −z+2; (ii) x−1, y, z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O7—H7o···O1wiii | 0.82 | 1.75 | 2.55 (1) | 166 |
O8—H8o···O1 | 0.82 | 2.01 | 2.815 (8) | 168 |
O1w—H1w···O1iv | 0.82 | 1.98 | 2.797 (8) | 171 |
O1w—H2w···O8 | 0.82 | 2.11 | 2.93 (1) | 172 |
Symmetry codes: (iii) x−1, y, z; (iv) −x+1, −y+2, −z+1. |
The present study on the title compound, (I), follows reports on the transition metal derivatives of 3-(4-carboxylatophenoxy)propionic acid. These (Kong et al., 2007a,b) describe the isostrutural manganese(II) and cobalt(II) adducts with 2,2'-bipyridine. With cadmium nitrate as reactant and by using a hydrothermal method, part of the carboxylic acid is hydrolyzed to give 4-hydroxybenzoic acid, which is then incorporated into the crystal structure (Fig. 1). Topologically, a double ribbon polyer is formed (Fig. 2).
The cadmium(II) atom in (I) exists in a seven-coordinate CdN2O5 enviroment (Fig. 3) that approximates to a monocapped octahedron (Table 1) and a network of O—H···O hydrogen bonds (Table 2) helps to consolidate the structure.